Method Validation for SPE Applied to Determination of PAH in Petroliferous Industry Effluent Water (original) (raw)
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Advances in Applied Science Research, 2014
A simple method of extraction and determination of sixteen priority polycyclic aromatic hydrocarbons (PAHs) from waste water and sediment using high performance liquid chromatography (HPLC) has been validated with limits of detection (LOD) and limits of quantification (LOQ), method recovery and reproducibility and other factors. HPLC parameters, such as mobile phase composition and flow standardized for determination of PAHs using ultra violetdiode array detector (UV-DAD). PAH extraction was carried out by liquid-liquid and Ultrasonication using dichloromethane and acetone/hexane solvents for water and sediment, respectively. Silica gel column chromatography was carried out for extract clean-up. Linearity of calibration curves was good for all sixteen PAH (R 2 , 0.991-0.996) in the concentration range 2.5-300 ppb. Analysis of standard spiked water and sediment samples resulted in good recoveries between 78-100 % and 82-106 %, respectively. The estimated LOD and LOQ ranged between 0.01-0.51 ppb and 0.03-1.71 ppb, respectively. The method described has been used for determination of the sixteen PAHs contents in water and sediment samples collected from municipal drains.
Trace levels of PAH pollutants are difficult to detect in water samples due to their low solubility. During this study, SPE method was used to improve the detection of the PAH analytes. A Visipre SPE vacuum manifolds sample preparation method was used to clean-up the river water samples before analysis. Twelve samples were simultaneously extracted via the unit. This method is generally faster and significantly increases sample throughput, while decreasing sample preparation hands-on time which is common for methods such as liquid-liquid extraction. An Agilent 1100 Series High Performance Liquid Chromatography (HPLC) was used to analyze trace levels of PAH compounds in river water samples before and after SPE treatment. Chromatograms of samples which were analyzed before treatment with the SPE method were simple, lacked details and could be mistaken as uncontaminated. However, after sample treatment, new peaks appeared which were well separated and relatively easier to identify when ...
Polycyclic aromatic hydrocarbons (PAHs) are major organic pollutants in the environment , which are toxic to humans and biota, given their carcinogenic, mutagenic and tera-togenic nature. In this chapter, we carried out an overview of the sources and toxicity of PAHs, their common analytical methods of determination in the water and sediment samples , and also their global trend of distribution, with a view to provide baseline guidance for relevant control authorities. The choice methods for determining these contaminants are high-performance liquid chromatography (HPLC) with UV/fluorescence detectors and GC/MS. Mass spectrometer coupled with GC is preferred because it offers robust identification of the analyte compounds both by retention time and mass spectrum, with additional structural information. Results collated revealed an extensive distribution of PAHs with total mean concentrations ranging from 0.0003 to 42,350 μg/L in water and 0 to 1.266 × 10 9 μg/kg (dw) in the sediment. PAHs in the two environmental matrices were much higher in the regions with intense oil exploration, shipping and industrial activities. It is therefore necessary to regularly monitor their levels in the aquatic environment, so as to provide mitigation options that will prevent risk to humans and aquatic animals.
Chimica et Natura Acta, 2022
Clean water is vital in the creation of energy and sustenance of life. However, the pollution of water and the absence of potable water are global problems resulting from agricultural and industrial activities. We have witnessed significant growth in the pollution of water by organic compounds like PAH. Experts have made an effort to establish favorable techniques for the treatment of PAH polluted water. These techniques are either thermal, biological, physical or chemical. Bioremediation, chemical oxidation, solid-phase extraction, coagulation, photocatalytic degradation and adsorption using graphenes, mesoporous silica and agricultural wastes are techniques that are already in use in the field treatment of PAHs while electrokinetic remediation and nanoremediation are still in their developmental stage. Several reviews on the treatment of sediments and soils contaminated with PAHs have been published, but only a few reviews center mainly on the removal of PAHs in water. Therefore, this review aims to provide information on the techniques used in the treatment of water contaminated with PAHs. Techniques that are already in use and those that are in their developmental stage were reviewed. The successes of these methods, limitations, constraints and field procedures were analyzed and this will help to inform decision making.
Monitoring of Polycyclic Aromatic Hydrocarbons in Surface Water of Shatt Al-Hilla River
Asian Journal of Chemistry, 2014
Polycyclic aromatic hydrocarbons (PAHs) refer to hydrocarbons containing two or more fused aromatic rings. All PAHs compounds are neutral and non-polar and they have high stability. All of them having high melting points and low vapor pressures and water solubility. Generally, the solubility and volatility of PAHs compounds are decrease and hydrophobicity increase with an increase in the number of fused aromatic rings 1. Fires and agriculture fires, fossil fuels burning, metalprocessing facilities, coke oven and internal burning engines in motor vehicles 2 can produce these compounds. The delocalization of π electron made these compounds exhibit high stability and low water solubility, leading to their accumulation in food chains 3. US Environmental Protection Agency (EPA), US Food and Drug Administration (FDA), National Oceanic Atmospheric Administration (NOAA) and the European Union Priority pollutants are listed PAHs as pollutant because of their mutagenic and carcinogenic properties 4-6. The procedures of enrichment and clean up are usually required prior determination of PAHs. There are several reports mention the application of solid phase extraction on the pre concentration of PAHs
Special Issue 1) Page 44 DETERMINATION OF POLYCYCLIC AROMATIC HYDROCARBONS (PAHS)
2020
The Gomti river, one of the major tributaries of the river Ganga serves as one of the major source of drinking water for the Lucknow City, the State capital of Uttar Pradesh, India. The river receives the untreated wastewater and effluents from Lucknow city directly in its course through more than 25 drains. Polycyclic aromatic hydrocarbons have been identified as exhibiting toxic/hazardous properties.Our study shows that Gomti river is highly contaminated with PAHs and poses high risk to the aquatic life. The study area covers seven different locations. Grab samples of water and bed sediments were collected from each of the locations in the month of November and December. Total PAHs in water at all the seven locations studied ranged between0.467-5.342 µg/l. In the river water the most abundant hydrocarbon was acenaphthene followed by acenaphthene. The most abundant hydrocarbon among all the analysed hydrocarbon in the river sediments was acenaphthene.
Journal of Chromatography A, 2006
A robust procedure for the determination of 16 US EPA PAHs in both aqueous (e.g. wastewaters, industrial discharges, treated effluents) and solid samples (e.g. suspended solids and sludge) from a wastewater treatment plant (WWTP) is presented. Recovery experiments using different percentages of organic modifier, sorbents and eluting solvent mixtures were carried out in Milli-Q water (1000 mL) spiked with a mixture of the PAH analytes (100 ng/L of each analyte). The solid phase extraction (SPE) procedures applied to spiked waste water samples (1000 mL; 100 ng/L spiking level) permitted simultaneous recovery of all the 16 PAHs with yields >70% (6-13% RSD). SPE clean up procedures applied to sewage and stabilized sludge extracts, showed percent recoveries in the range 73-92% (7-13% RSD) and 71-89% (7-12% RSD) respectively. The methods were used for the determination of PAHs in aqueous and solid samples from the WWTP of Fusina (Venice, Italy). Mean concentrations, as the sum of the 16 PAHs in aqueous and suspended solid samples, were found to be approx. in the 1.12-4.62 µg/L range. Sewage and stabilized sludge samples contained mean PAH concentrations, as sum of 16 compounds, in the concentration range of 1.44-1.26 mg/kg, respectively. Extraction and clean up procedures for sludge samples were validated using EPA certified reference material IRM-104 (CRM No.912). Instrumental analyses were performed by coupling HPLC with UV-diode array detection (UV-DAD) and fluorescence detection (FLD).
Journal of Al-Nahrain University Science, 2014
In this paper sixteen polycyclic Aromatic Hydrocarbons (PAHs) were estimated in eight sites along Diyala River where entering Baghdad province until flows into Tigris River, (PAHs) organic compound dscontain two or more fused rings. Some of these compounds are classified as carcinogenic and mutagenic pollutants. Solid Phase extraction was used in this work to concentrate PAHs in water samples using Sep-back C18 showed percentage recoveries between (82-97) percent. High Performance Liquid Chromatography (HPLC) with UV-Vis detector was used for determination of PAHs. The result of PAHs concentrations were found in the water samples range between (zero-186.86)ng/ml. According to our results sites number one, two, six, seven and eight have the least values of total PAHs concentration with 10.8, 12.0, 39.3, 30.7 and 14.9 ng/ml respectively, while, three, four and five sites have a largepolluted with 396.5, 660.9 and 189.5 ng/ml respectivelybecause these sites are near pollutants sources. Naphthalene, Anthracene and Fluoranthene with total concentrations415.8, 259.2 and 286.4 ng/ml respectively, compounds Benzo [a] pyrene and Dibenz [a, h] anthracene arenot detected in all sites.